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A kind of preparation method of continuous production of diethylformamide

A technology of diethylformamide and production method, which is applied in the preparation of carboxylic acid amides, the preparation of organic compounds, chemical instruments and methods, etc., can solve the problems of large reactors, increased separation energy consumption and material consumption, and ignition, etc., Achieve the effect of simple industrial scale-up, low material consumption and high yield

Active Publication Date: 2016-05-18
MAIQI CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These defects will result in the need to use larger reactors, and are prone to extreme hazards such as fire, separation energy consumption and material consumption increase

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] A preparation method for continuous production of diethylformamide. In a closed tubular reactor filled with a heterogeneous catalyst, diethylamine and methyl formate are mixed and converted into diethylformamide through amidation reaction , After refining the finished product diethyl formamide.

[0028] The reaction conditions are: the molar ratio of diethylamine to methyl formate is 1.0~1.1:1.0, and the liquid phase space velocity is 15.0h -1 , The reaction temperature is controlled to 80℃, and the reaction pressure (gauge pressure) is normal pressure to 0.2MPa. The chemical composition of the heterogeneous catalyst is: a mixture of alumina, magnesia and zirconia.

[0029] The heterogeneous catalyst has a strip shape, and the maximum length dimension is 2 mm.

[0030] The water content of the diethylamine is 0.2wt%.

[0031] The methanol content in methyl formate is 0.1% by weight.

[0032] Measure the export products, the conversion rate of diethylamine is 99.3%, DEF selectiv...

Embodiment 2

[0034] A preparation method for continuous production of diethylformamide. In a closed tubular reactor filled with a heterogeneous catalyst, diethylamine and methyl formate are mixed and converted into diethylformamide through amidation reaction , After refining the finished product diethyl formamide.

[0035] The reaction conditions are: the molar ratio of diethylamine to methyl formate is 1.0~1.1:1.0, the liquid phase space velocity is 10.0h-1, the reaction temperature is controlled at 60°C, and the reaction pressure (gauge pressure) is normal pressure ~ 0.2MPa. The chemical composition of the heterogeneous catalyst is: a mixture of titanium oxide and calcium oxide.

[0036] The heterogeneous catalyst has a spherical shape with a maximum length of 3 mm.

[0037] The water content of the diethylamine is 0.1wt%.

[0038] The methanol content in methyl formate is 0.05wt%.

[0039] Measure the export products, the conversion rate of diethylamine is 99.5%, DEF selectivity is close to 100...

Embodiment 3

[0041] A preparation method for continuous production of diethylformamide. In a closed tubular reactor filled with a heterogeneous catalyst, diethylamine and methyl formate are mixed and converted into diethylformamide through amidation reaction , After refining the finished product diethyl formamide.

[0042] The reaction conditions are: the molar ratio of diethylamine to methyl formate is 1.0~1.1:1.0, and the liquid phase space velocity is 5.0h -1 , The reaction temperature is controlled at 50℃, and the reaction pressure (gauge pressure) is normal pressure ~ 0.2MPa. The chemical composition of the heterogeneous catalyst is: a mixture of alumina, magnesia and zirconia.

[0043] The heterogeneous catalyst is spherical, and the maximum length dimension is 1.5 mm.

[0044] The water content of the diethylamine is 0.4wt%.

[0045] The methanol content in methyl formate is 0.08wt%.

[0046] Measure the export products, the conversion rate of diethylamine is 99.5%, DEF selectivity is close...

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Abstract

The invention relates to a method for producing diethylformamide. The invention relates to a preparation method for continuous production of diethylformamide, which comprises the following steps: mixing diethylamine and methyl formate, converting to diethylformamide through an amidation reaction, and refining to obtain the finished product diethylformamide; wherein the mol ratio of diethylamine to methyl formate is 1.0-1.1: 1.0, space velocity of the liquid phase is 1.0-20.0h<-1>, the reaction temperature is controlled at 10-80 DEG C, and the reaction pressure (gauge pressure) is between normal pressure and 0.2MPa. The method has the advantages of high yield, because that high mol ratio of methyl formate to diethylamine is not required, diethylamine conversion rate is high, and the material consumption of whole process is little. The preparation method makes DEF production to serialization, so that the production efficiency of the process is increased, and the investment and production cost can be greatly reduced.

Description

Technical field: [0001] The invention relates to a production method of diethylformamide. Background technique: [0002] N,N-Diethylformamide (DEF), English name is N, N-Diethylformamide, abbreviated as DEF; molecular formula is C 5 H 11 NO; molecular weight is 101.15; density is 0.9049, boiling point is 177~178℃, it is a colorless, transparent, low-density, high-boiling point polar organic solvent, miscible with water, alcohol, ether, ketone, benzene, etc., and has strong solubility. It can dissolve many organic polymers, such as polyacrylonitrile, urethane prepolymer, PVC, vinylidene chloride-vinyl chloride copolymer, polyvinyl formal, polyimide and other high-molecular polymers, so DEF can As an industrial solvent, it replaces N,N-dimethylformamide (DMF), and has far less toxic and side effects than DMF. In addition, DEF also has potential application value in the field of fiber synthesis and pharmaceutical synthesis. [0003] Liu Xingquan et al. disclosed a DEF synthesis meth...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C233/03C07C231/02
Inventor 宋国全肖强杨理闫广学
Owner MAIQI CHEM CO LTD
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